CN109400935B - Super-hydrophobic surface with bionic pore structure and preparation method thereof - Google Patents
Super-hydrophobic surface with bionic pore structure and preparation method thereof Download PDFInfo
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- CN109400935B CN109400935B CN201811108909.3A CN201811108909A CN109400935B CN 109400935 B CN109400935 B CN 109400935B CN 201811108909 A CN201811108909 A CN 201811108909A CN 109400935 B CN109400935 B CN 109400935B
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Abstract
The invention provides a super-hydrophobic surface with a bionic pore structure and a preparation method thereof, belongs to the technical field of functional materials, and particularly relates to a preparation method of the surface with the bionic pore structure. The method comprises the following steps: preparing a Polydimethylsiloxane (PDMS) film, preparing an Ethylenediamine (EDA) aqueous solution, swelling the PDMS film in tetraethyl orthosilicate (TEOS), floating the swelled PDMS film on the surface of the EDA aqueous solution, performing catalytic hydrolytic polycondensation, performing heat treatment and the like. The bionic pores on the super-hydrophobic surface are of a micron-scale structure, a nano structure is not required to be constructed, low-surface-energy substances such as fluorosilane and the like are not required to be secondarily modified, the preparation method is ingenious, the raw materials are cheap, the operation is simple, and the energy consumption is low. The super-hydrophobic surface with the bionic pore structure has the characteristics of no water, no acid, no alkali and super-oleophylic property, and is wide in application.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a super-hydrophobic surface with a bionic pore structure and a preparation method thereof.
Background
Due to the special wetting property of the super-hydrophobic surface, the super-hydrophobic surface has a good application prospect in daily life and has urgent needs in high-tech fields such as national defense, military industry, shipbuilding and the like. In recent years, people study and construct similar multi-scale micro-nano interfaces by simulating the surface structures of animals and plants with special wettability such as lotus leaves, prepare a plurality of super-hydrophobic and super-hydrophilic interface materials, and realize that the wettability of the solid surface is the result of controlling the surface micro-nano structure and chemical composition together. The design of the super-hydrophobic surface microstructure is divided into a single-scale geometric structure and a multi-scale fractal geometric structure, and the current single-scale geometric structure comprises the following components: square column array structure, trapezoidal column array structure, hemispherical top column array structure, cone array structure, cylindrical array structure, spherical array structure, and the like. Biomimetic pore structures have not been used for the preparation of superhydrophobic surfaces.
PDMS is widely used for the preparation and research of superhydrophobic surfaces as an organic silicon polymer with high flexibility, good biocompatibility, no toxicity and high chemical stability. The preparation method of the PDMS super-hydrophobic surface comprises the following steps: template method, photoetching, plasma method, cladding method, organic-inorganic doping method, hydrothermal method and the like. Expensive equipment such as laser, plasma, spraying, spin coating and the like is used in photoetching, plasma methods, coating methods and the like, the template method is greatly influenced by the template structure and the operation of the stripping step, and the cost of the used fluorosilane is high, so that the method is not beneficial to industrial popularization and application. Therefore, the development of a preparation method of the super-hydrophobic surface which is simple, low in cost, free of water, acid and alkali and super-oleophylic is still urgent.
Disclosure of Invention
The invention aims to provide a super-hydrophobic surface with a bionic pore structure, which has the characteristics of no water, no acid, no alkali and super-oleophylic property.
The invention further aims to provide a preparation method of the super-hydrophobic surface with the bionic pore structure.
The invention also aims to realize the super-hydrophobic property of the surface by adopting cheap raw materials and a simple method at normal temperature and normal pressure without constructing a nano structure or modifying low-surface-energy substances such as fluorosilane and the like for the second time.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a super-hydrophobic surface with a bionic pore structure comprises the following steps:
(1) preparing a PDMS film;
(2) preparing an EDA aqueous solution;
(3) swelling the PDMS film prepared in the step (1) in TEOS;
(4) floating the swelled PDMS film on the surface of the EDA aqueous solution to perform catalytic hydrolysis polycondensation, taking out and cleaning the PDMS film with deionized water;
(5) and (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment to obtain the super-hydrophobic surface with the bionic pore structure. In the step (1), the preparation method of the PDMS film is as follows: and the mass ratio of the PDMS to the curing agent is 8:1-12:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 60-95 ℃ for 3-12 h to obtain the PDMS membrane.
Preferably, in the step (2), the EDA aqueous solution is prepared by uniformly mixing EDA and deionized water according to a volume ratio of 5: 100-15: 100, and then sealing and storing.
Preferably, in the step (3), the PDMS film is immersed in TEOS, and is subjected to swelling treatment at 25-40 ℃ for 0.5-24 h, and then is taken out and the residual TEOS on the surface is drained.
Preferably, in the step (4), the PDMS film floats on the surface of the EDA aqueous solution in the step (2), the container is sealed, the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 6-24 h, and the reaction temperature is 20-35 ℃.
Preferably, in the step (5), the heat treatment temperature is 45-120 ℃, and the treatment time is 1-24 h.
According to the technical scheme, a crosslinked and cured PDMS membrane is placed into TEOS for swelling, then the crosslinked and cured PDMS membrane floats on the surface of an EDA (electronic design automation) aqueous solution, TEOS micro droplets naturally separated out of the surface of the PDMS form a silicon dioxide gel micro cavity through hydrolysis-condensation-polymerization under the action of ethylenediamine steam and water vapor, the micro cavity is broken through heat treatment to form a super-hydrophobic surface with a micron-scale bionic pore structure, the pore radius (R) of the bionic pores is 0.50-3.0 mu m, the hemisphere radius (R) is 1.0-8.0 mu m, and the center distance (D) of the bionic pores is 2.0-10.0 mu m. The super-hydrophobic water surface with the bionic pore structure has a contact angle to water of more than 160 degrees, a contact angle to oil substances such as toluene, xylene, butyl acetate, dichloromethane, trichloromethane and the like of 0 degree, a contact angle to diesel oil of less than 10 degrees, a contact angle to acid of more than 150 degrees, a contact angle to alkali of more than 160 degrees and a contact angle to salt of more than 160 degrees.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, PDMS is used as a substrate, a silicon dioxide gel micro-cavity is formed through hydrolysis-condensation-polymerization at normal temperature and pressure, and then the micro-cavity is broken through heat treatment to form a bionic pore so as to obtain a super-hydrophobic surface, the preparation method is ingenious, the raw materials are cheap, the operation is simple, and the energy consumption is low;
2. according to the super-hydrophobic surface with the bionic pore structure, the bionic pores are of a micron-scale structure, a nano structure is not required to be constructed, low-surface-energy substances such as fluorosilane and the like are not required to be secondarily modified, and the super-hydrophobic surface with the water contact angle larger than 160 degrees is obtained;
3. the super-hydrophobic surface with the bionic pore structure is not sticky with water, acid and alkali, is super-oleophilic, and has wide application.
Drawings
FIG. 1 is a scanning electron micrograph of a superhydrophobic surface with a biomimetic pore structure, magnified 1000 times;
FIG. 2 is a scanning electron micrograph of a superhydrophobic surface with a biomimetic pore structure, magnified 5000 times;
FIG. 3 is a scanning electron micrograph of the hydrophobic surface of comparative example 1, magnified 1000 times;
fig. 4 is a scanning electron micrograph of the hydrophobic surface in comparative example 1, magnified 10000 times.
Detailed Description
In order to make the present invention easier to understand, the following examples will further illustrate the present invention, but the scope of the present invention is not limited to these examples.
The method for measuring the contact angle of the super-hydrophobic surface with the bionic pore structure comprises the following steps:
the invention uses a video contact angle tester to measure the contact angle: 5 mu L of deionized water, acid solution, alkali solution, salt solution and oil substance are used as liquid drops, and after the liquid drops are stabilized on the surface of the film for 30s, the contact angle is measured by adopting an angulometry. Generally, the contact angle of water is more than 150 degrees, the super-hydrophobic property is realized, and the contact angle of oil is less than 10 degrees, the super-oleophylic property is realized.
Example 1
(1) And the mass ratio of the PDMS to the curing agent is 10:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 95 ℃ for 5h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 10:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 25 ℃ for 0.5h, removed and the surface residual TEOS was drained.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 10h, the reaction temperature is 30 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment at 120 ℃ for 1h to obtain the super-hydrophobic surface with the bionic pore structure.
The microstructure of the super-hydrophobic surface is shown in a figure 1 and a figure 2, the bionic air holes are of a micron-sized structure, the radius (R) of the air holes of the bionic air holes is 0.50-3.0 mu m, the radius (R) of hemispheres is 1.0-8.0 mu m, and the center distance (D) of the bionic air holes is 2.0-10.0 mu m; the contact angle measurement results are: the contact angle to water is 163.9 degrees, the contact angle to toluene, xylene, butyl acetate, dichloromethane and chloroform is 0 degree, the contact angle to diesel oil is less than 10 degrees, the contact angle to acid is 151.4 degrees, the contact angle to alkali is 161.4 degrees, the contact angle to salt is 162.6 degrees, and the characteristics of super-hydrophobicity, super-oleophylicity, non-stick to acid and non-stick to alkali are presented.
Comparative example 1
(1) And the mass ratio of the PDMS to the curing agent is 10:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 95 ℃ for 5h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 10:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 25 ℃ for 3.0h, removed and the surface residual TEOS was drained.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 5h, the reaction temperature is 40 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment at the temperature of 95 ℃ for 1h to obtain the hydrophobic surface. The microstructure of the hydrophobic surface is shown in fig. 3 and 4, the contact angle to water is 141.1 ± 2 °, and the super-hydrophobicity is not reached.
Example 2
(1) And the mass ratio of the PDMS to the curing agent is 8:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 95 ℃ for 3h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 8:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 30 ℃ for 1.0h, removed and the surface residual TEOS was drained.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 12h, the reaction temperature is 30 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment at the temperature of 45 ℃ for 24 hours to obtain the super-hydrophobic surface with the bionic pore structure.
Example 3
(1) And the mass ratio of the PDMS to the curing agent is 12:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 60 ℃ for 12h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 15:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 30 ℃ for 3.0h, removed and the surface residual TEOS was drained.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 6h, the reaction temperature is 35 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment, wherein the treatment temperature is 95 ℃, and the treatment time is 6 hours, so as to obtain the super-hydrophobic surface with the bionic pore structure.
Example 4
(1) And the mass ratio of the PDMS to the curing agent is 10:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 80 ℃ for 6h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 5:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 30 ℃ for 24h, removed and drained of the surface residual TEOS.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 24h, the reaction temperature is 20 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment at the temperature of 60 ℃ for 8 hours to obtain the super-hydrophobic surface with the bionic pore structure.
Example 5
(1) And the mass ratio of the PDMS to the curing agent is 9:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 70 ℃ for 8h to obtain the PDMS membrane.
(2) Preparing an EDA aqueous solution, uniformly mixing EDA and deionized water according to the volume ratio of 10:100, and sealing for storage.
(3) The PDMS membrane was immersed in TEOS, swollen at 30 ℃ for 12h, removed and drained of the surface residual TEOS.
(4) And (3) floating the PDMS film on the surface of the EDA aqueous solution in the step (2), sealing the container, wherein the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 20h, the reaction temperature is 30 ℃, and then taking out the PDMS film and cleaning the PDMS film with deionized water.
(5) And (4) placing the PDMS membrane treated in the step (4) in an oven for heat treatment at the temperature of 110 ℃ for 2h to obtain the super-hydrophobic surface with the bionic pore structure.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. The super-hydrophobic surface is characterized by having a bionic air hole structure, wherein the bionic air hole structure is a micron-sized structure, the air hole radius (R) of a bionic air hole is 0.50-3.0 mu m, the hemisphere radius (R) is 1.0-8.0 mu m, and the center-to-center distance (D) of the bionic air hole is 2.0-10.0 mu m.
2. The superhydrophobic surface of claim 1, wherein: the contact angle of the methanol gasoline to toluene, xylene, butyl acetate, methylene dichloride and chloroform is 0 degree, the contact angle to diesel oil is less than 10 degrees, the contact angle to acid is more than 150 degrees, and the contact angles to water, alkali and salt are all more than 160 degrees.
3. A preparation method of a super-hydrophobic surface with a bionic pore structure is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a PDMS film;
(2) preparing an EDA aqueous solution;
(3) swelling the PDMS film prepared in the step (1) in TEOS;
(4) floating the swelled PDMS film on the surface of the EDA aqueous solution to perform catalytic hydrolysis polycondensation, taking out and cleaning the PDMS film with deionized water;
(5) and (3) placing the PDMS membrane treated in the step (4) in an oven for heat treatment to obtain the super-hydrophobic surface with a bionic air hole structure, wherein the bionic air hole structure is a micron-sized structure, the air hole radius (R) of the bionic air hole is 0.50-3.0 mu m, the hemisphere radius (R) is 1.0-8.0 mu m, and the center distance (D) of the bionic air hole is 2.0-10.0 mu m.
4. The method for preparing the superhydrophobic surface with the bionic pore structure according to claim 3, wherein the method comprises the following steps: and the mass ratio of the PDMS to the curing agent is 8:1-12:1, stirring for 5min, removing bubbles in vacuum, pouring into a mold, and curing at 60-95 ℃ for 3-12 h to obtain the PDMS membrane.
5. The method for preparing the superhydrophobic surface with the bionic pore structure according to claim 3, wherein the method comprises the following steps: in the step (2), the EDA aqueous solution is prepared by uniformly mixing EDA and deionized water according to the volume ratio of 5: 100-15: 100, and then sealing and storing.
6. The method for preparing the superhydrophobic surface with the bionic pore structure according to claim 3, wherein the method comprises the following steps: in the step (3), the PDMS film is immersed in TEOS, is subjected to swelling treatment for 0.5-24 h at 25-40 ℃, and is taken out and the residual TEOS on the surface is drained.
7. The method for preparing the superhydrophobic surface with the bionic pore structure according to claim 3, wherein the method comprises the following steps: in the step (4), the PDMS film floats on the surface of the EDA aqueous solution in the step (2), the container is sealed, the surface facing the air is a super-hydrophobic surface, the catalytic hydrolysis and polycondensation time is 6-24 h, and the reaction temperature is 20-35 ℃.
8. The method for preparing the superhydrophobic surface with the bionic pore structure according to claim 3, wherein the method comprises the following steps: in the step (5), the heat treatment temperature is 45-120 ℃, and the treatment time is 1-24 h.
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| CN105413994A (en) * | 2015-12-15 | 2016-03-23 | 大连理工大学 | Preparation method for super-hydrophobic surface with bionic micro-nano composite structure |
| CN108329499A (en) * | 2018-01-25 | 2018-07-27 | 合肥中科富华新材料有限公司 | A kind of water resistant oil resistant plastic preparation method and its water resistant oil resistant plastics |
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| CN105413994A (en) * | 2015-12-15 | 2016-03-23 | 大连理工大学 | Preparation method for super-hydrophobic surface with bionic micro-nano composite structure |
| CN108329499A (en) * | 2018-01-25 | 2018-07-27 | 合肥中科富华新材料有限公司 | A kind of water resistant oil resistant plastic preparation method and its water resistant oil resistant plastics |
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